ASTM D5310-10e1
(Test Method)Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography
Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography
SIGNIFICANCE AND USE
This test method is suitable for the general quantitative analysis of commercial tar acid mixtures. It may be used as a tool for quality control and specification purposes by producers and users.
SCOPE
1.1 This test method covers the quantitative determination of phenol and certain homologues of phenol in tar acid and cresylic acid mixtures using capillary gas chromatography. It is a normalization test method that determines homolog distribution but is not an absolute assay since it does not account for water or other compounds not detected by a flame ionization detector.
1.2 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.
General Information
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Standards Content (Sample)
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Designation: D5310 − 10
StandardTest Method for
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Tar Acid Composition by Capillary Gas Chromatography
This standard is issued under the fixed designation D5310; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
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ε NOTE—The title of Figure 3 was corrected editorially in February 2010.
1. Scope* E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
1.1 This test method covers the quantitative determination
2.2 Other Documents:
of phenol and certain homologues of phenol in tar acid and
OSHA Regulations, 29 CFR paragraphs 1910.1000, and
cresylic acid mixtures using capillary gas chromatography. It is
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1910.1200
a normalization test method that determines homolog distribu-
tion but is not an absolute assay since it does not account for
3. Terminology
water or other compounds not detected by a flame ionization
3.1 For definition of terms used in this test method see
detector.
Terminology D4790.
1.2 In determining the conformance of the test results using
this method to applicable specifications, results shall be
4. Summary of Test Method
rounded off in accordance with the rounding-off method of
4.1 The sample composition is determined by capillary gas
Practice E29.
chromatography. The weight percent composition is calculated
1.3 The values stated in SI units are to be regarded as from the ratio of the individual peak areas to the total area of
standard. No other units of measurement are included in this
all peaks using appropriate response factors determined for
standard. each component by means of a calibration sample.
1.4 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 This test method is suitable for the general quantitative
responsibility of the user of this standard to establish appro-
analysis of commercial tar acid mixtures. It may be used as a
priate safety and health practices and determine the applica-
toolforqualitycontrolandspecificationpurposesbyproducers
bility of regulatory limitations prior to use. For specific hazard
and users.
statements, see Section 8.
6. Apparatus
2. Referenced Documents
2 6.1 Chromatograph—Agaschromatographcompatiblewith
2.1 ASTM Standards:
capillary columns, equipped with inlet splitter and high tem-
D3852 Practice for Sampling and Handling Phenol, Cresols,
perature flame ionization detector. Typical Operating Condi-
and Cresylic Acid
tions are given in Table 1.
D4790 Terminology ofAromatic Hydrocarbons and Related
Chemicals 6.2 Peak Integrator—Electronic integration is recom-
D6809 Guide for Quality Control and Quality Assurance mended.
Procedures for Aromatic Hydrocarbons and Related Ma-
6.3 Recorder, with full scale response time of1sor less.
terials
6.4 Microsyringe, capacity of 1 µL.
6.5 Capillary Column—Any column capable of resolving
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This test method is under the jurisdiction of ASTM Committee D16 on
all components of interest. Prepared columns are commercially
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
available from chromatography supply houses. Chromato-
Subcommittee D16.02 on Oxygenated Aromatics.
grams from three columns are presented in Fig. 1, Fig. 2, and
Current edition approved Jan. 1, 2010. Published January 2010. Originally
approved in 1994. Last previous edition approved in 2004 as D5310 – 00 (2004). Fig. 3. Peak identification is given in Table 2.
DOI: 10.1520/D5310-10E01.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
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contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. www.access.gpo.gov.
*A Summary of Changes section appears at the end of this standard
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D5310 − 10
TABLE 1 Typical Chromatographic Operating Conditions
Cyanopropyl 25 %, Phenyl 25 %, Dimethyl 95 %, Diphenylpolysiloxane
Column Liquid Phase Diisodecyl Phthalate
Methylpolysiloxane 50 %, Bonded Phase 5 %, Bonded Phase
Column Fused Silica Fused Silica Fused Silica
Column length, m 30 25 30
Column ID, mm 0.25 0.22 0.25
Film thickness,µ m 0.2 0.2 0.25
Column temperature,° C 100 100 105
Detector temperature,° C 200–275 200–275 200–275
Injection block temperature, °
...
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